Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop (VASEME-SFO) was used for preconcentration and speciation of antimony (ΙΙΙ,V) followed by electrothermal atomic absorption spectrometry (ETAAS). In this procedure, Triton X-114was used as emulsifier and 1-undecanol was used as extraction solvent. This method is based on the complexation of Sb(ΙΙΙ) with dithizone (as complexing agent) at pH2 and extraction of the resulting hydrophobic complex into the extraction solvent (1-undecanol) with vortex-assisted liquid phase microextraction, whereas Sb(V) remained in solution. Sb(ΙΙΙ) in extraction solvent was directly analyzed by ETAAS after dilution with ethanol, and Sb(V) was calculated by subtracting Sb(ΙΙΙ)fromthe total antimony after reducing Sb(V) to Sb(ΙΙΙ)byLcysteine. Under the optimized condition, the calibration curve was linear in the range of 0.4–8μgL −1 of Sb(ΙΙΙ) with a correlation coefficient of 0.9995. The detection limit based on three times of the standard deviation of the blank (n=8) was 0.09μgL −1. The validation and the recovery of the proposedmethodwere performed by the analysis of a certified referencematerial and spikemethod. The obtained results were in very good agreements with certified values. The proposed method was successfully applied for the determination of antimony species at trace levels in different water samples.

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